HRID1907352
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
CONDITIONS
反应条件
- 温度
- 105 °C
PROCEDURE
实验过程
8.78 g of ethyl [2-imino-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyridin-1-yl]acetate hydrobromide in 20 ml of POCl3 are placed in a round-bottomed flask. The reaction mixture is heated at 105° C. for 16 h, cooled to ambient temperature and concentrated under reduced pressure. The residue is taken up between dichloromethane and water at 0° C., and a 30% aqueous solution of NH4OH is added until a basic pH is obtained. The organic phase is separated, dried over magnesium sulphate and concentrated under reduced pressure. 4.3 g of compound are obtained.
WORKUP
后处理
- temperaturecooled to ambient temperature
- concentrationconcentrated under reduced pressure
- customis taken up between dichloromethane and water at 0° C.
- additiona 30% aqueous solution of NH4OH is added until a basic pH
- customis obtained
- customThe organic phase is separated
- dry with materialdried over magnesium sulphate
- concentrationconcentrated under reduced pressure